Physics Procedia

Volume 75, 2015, Pages 1396–1403

20th International Conference on Magnetism

Study of AC magnetic properties and core losses of

Fe/Fe3O4-epoxy resin soft magnetic composite
Laxminarayana T. A.1*, Subhendu Kumar Manna2, Fernandes B. G.3
and Venkataramani N.1†
1
Department of Metallurgical Engineering and Materials Science, Indian Institute of Technology
Bombay, Mumbai, India, 400076.
2
Department of Physics, Indian Institute of Technology Madras, Chennai, India, 600036.
3
Department of Electrical Engineering, Indian Institute of Technology Bombay, Mumbai, India,
400076.

Abstract

Soft Magnetic Composites (SMC) were prepared by coating of nanocrystalline Fe 3O4 particles,
synthesized by co-precipitation method, on atomized iron powder of particle size less than 53 µm in
size using epoxy resin as a binder between iron and Fe3O4. Fe3O4 was chosen, for its high electric
resistivity and suitable magnetic properties, to keep the coating layer magnetic and seek improvement
to the magnetic properties of SMC. SEM images and XRD patterns were recorded in order to
investigate the coatings on the surface of iron powder. A toroid was prepared by cold compaction of
coated iron powder at 1050 MPa and subsequently cured at 150˚C for 1 hr in argon atmosphere. For
comparison of properties, a toroid of uncoated iron powder was also compacted at 1050 MPa and
annealed at 600˚C for 2 hr in argon atmosphere. The coated iron powder composite has a resistivity of
greater than 200 μΩm, measured by four probe method. A comparison of Magnetic Hysteresis loops
and core losses using B-H Loop tracer in the frequency range 0 to 1500 Hz on the coated and uncoated
iron powder is reported.

Keywords: Soft Magnetic Composite, High frequency applications, Core losses

1 Introduction
Soft magnetic composites (SMC) are electrically insulated iron/iron alloy powders that may be
used for high frequency electrical applications due to low core losses and 3D magnetic flux
propagation capabilities [1-3]. Soft magnetic materials with high permeability and low losses are of
interest for high frequency (400 Hz to few KHz) and high speed electric motors. Sintered soft iron

*
E-mail: ta.laxminarayana@gmail.com
†
Corresponding author. Tel: +91-22-2576-7657
Email: ramani@iitb.ac.in

1396 Selection and peer-review under responsibility of the Scientific Programme Committee of ICM 2015

c The Authors. Published by Elsevier B.V.
doi:10.1016/j.phpro.2015.12.157
Study of AC magnetic properties and core losses ... Laxminarayana T. A. et al.

powder compacts are used for DC applications, for low frequency (few hundred Hz) applications
laminated steels are used [4, 5]. However, sintered iron compacts and laminated steel are not useful for
high frequency applications due to eddy current losses when used in AC magnetic fields. Soft ferrites
are used at high frequencies (few MHz to GHz) due to their high electrical resistivity. However
ferrites possess lower saturation induction in comparison with soft iron containing alloys. Electrically
insulated iron powders (SMC) with better magnetic properties and low core losses may hence be used
for applications in the frequency range few kHz. The electrical insulation on the iron powder particles
should lower the eddy current losses. The insulation layer characteristics need also be optimized for
better permeability and core losses [6-9]. Electrical insulations based on inorganic compound makes it
possible for high temperature heat treatments that may yield the better magnetic properties in the final
product in comparison to organic compound based insulations. This paper presents a study of SMC
prepared by insulating micrometer sized iron powder with uniform nano sized Fe3O4 particles and
epoxy resin.

2 Experimental Details

2.1 Materials

Atomized iron powder of the grade JIP (KIP) 304A, procured from JFE Steel Corporation Tokyo,
was first sieved and separated according to particle size. Iron powder with particle size of less than 53
µm (-270 ASTM mesh) was used for the composite preparation. For Fe3O4 preparation FeCl2.4H2O,
FeCl3 and NaOH pellets sourced from Merck India were used. Also for the Epoxy resin, Araldite® 506
epoxy resin and 4,4’-Methylenedianiline hardener supplied by Sigma Aldrich and Acros Organics
were used.

2.2 Fe3O4 preparation by co-precipitation method

The stoichiometry of the chemicals was determined by using the following equation.

2+ 3+ −
Fe + 2Fe + 8OH → Fe3O4 + 4H2O (1)

The reaction solution was prepared by dissolving 4.5 millimol of FeCl2.4H2O and 9 millimol of
FeCl3 in 100 ml distilled water followed by stirring at 80˚C under N2 gas atmosphere. 36 millimole of
NaOH were dissolved in 100 ml distilled water. The prepared NaOH solution was added drop by drop
into the reaction solution and the reaction was performed at 80˚C under N2 gas atmosphere, until black
precipitate of Fe3O4 was formed. The solution was decanted and the precipitate of Fe3O4 washed
several times using distilled water till chloride ions were removed. The prepared Fe3O4 particles were
in the range of 20-50 nm and were characterized by powder X-ray diffraction (XRD).

2.3 Composite preparation

A composite was prepared with volume percentages of iron, Fe 3O4 and epoxy resin in the ratio of
95, 2.5 and 2.5 respectively. First Araldite® 506 epoxy resin and 4, 4’-Methylenedianiline were
dissolved in acetone. 4,4’-Methylenedianiline is the hardener for the epoxy resin and the resin to
hardener ratio was maintained at 4:1 by weight. Fe3O4 nano powder was added into this followed by
stirring for uniform distribution of Fe3O4 nano particles and epoxy resin. Now the iron powder was
added to this mixture and stirred until all of the acetone evaporated. This resulted in the coating of

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Fe3O4 and epoxy resin on the iron powder. The coated iron powder was then dried and cured at 70ºC
in air.

A toroid of dimension outer diameter = 35 mm, inner diameter = 25 mm was compacted at 1050
MPa using the composite powder mixture. This toroid was post cured at 150˚C in argon atmosphere
for 2 hr. The coating on the iron powder was characterized by powder X-ray diffraction (XRD) and
scanning electron microscope imaging (SEM) techniques. For comparison of properties uncoated iron
powder was also compacted at 1050 MPa as a toroid of similar dimensions and annealed at 600ºC for
2 hr in argon atmosphere.

Toroids were wound with primary (400 turns) and secondary (300 turns) copper windings for
measurement of AC magnetic properties and core losses using a hysteresis loop tracer in the frequency
range 0-1500 Hz, made by Laboratorio Elettrofisico Walker LDJ Scientific, Italy. Resistivity of the
toroids was measured by the four probe method.

3 Results and Discussion

3.1 Insulating Layer Characterization

Figure 1: XRD patterns of the synthesized Fe3O4 and coated iron powder.
Figure 1 shows XRD patterns of coated iron powder composite and Fe3O4 powder samples. It can
be seen that, diffraction peaks of the coated iron are consistent with the standard pattern for Fe3O4
(JCPDS Card No: 019-0629) and iron (JCPDS Card No: 06-0696) respectively indicating that iron
powder was coated with Fe3O4. The XRD pattern of Fe3O4 showed very broad peaks, indicating the
ultra-fine nature and nano crystallite size of the synthesized particles. Cubic single phase nano
sized Fe3O4 powder had been obtained by the co-precipitation method.
The grain size of the Fe3O4 nanoparticles was calculated from the Scherrer formula:

λ
 ൌ Ⱦ…‘• θ (2)

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Study of AC magnetic properties and core losses ... Laxminarayana T. A. et al.

Where β is the full width at half maximum (FWHM), D is the grain size in nm, θ is the
corresponding Bragg angle , λ is the Cu-Kα X-ray wavelength (0.154 nm), and K is the shape
parameter which is taken as 0.89 for Fe3O4. The grain size, calculated using the highest intensity
peak (311) at 2θ = 35.4°, was 26 nm.

Figure 2: SEM images of (a) coated iron powder (b) coated iron powder surface (c) EDS analysis of coated
iron powder.

Figure 2 shows the SEM images of coated iron powder and the performed energy dispersed analysis.
We can see that iron powder is coated with nano sized Fe3O4 particles and that the coating is uniform.
Making coating of nano Fe3O4 particles directly on iron powder is quite difficult. The epoxy resin
binds the Fe3O4 nano particles to the iron surface and thus coats the iron powder. The epoxy resin
also leads to the agglomeration of nano Fe3O4 particles which is observed in the SEM images.
Figure 2(c) shows the EDS analysis of the Fe3O4 coated iron powder. The surface layer essentially
consists of iron, oxygen and carbon. EDS also shows the presence of platinum because of metallic
coating of the powder done before the SEM and EDS operation to reduce charging effects. Therefore
from the XRD patterns analysis, SEM images and EDS analysis it is seen that the iron powder is
coated uniformly with Fe3O4 nano particles.

3.2 DC Resistivity Measurement

Resistivity measurement of SMC is important to evaluate the insulation layer coated on iron
powder. Four probe method is preferable for measuring resistivity since iron is a good conductor. In
general resistivity measurement is done on rectangular bar or cylindrical sample of known dimension
with uniform cross-section area. Unlike rectangular bar or cylindrical sample toroid shape is a closed

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geometry with uniform cross-sectional area. For this the current probes are connected at any two
opposite points of the toroid that divide the toroid into two half portions (Figure 3(a)). The inner
lengths of the two half portions of the toroid (L1 & L2) are equal.

Figure 3: (a) Schematic diagram of toroid sample for resistivity measurement (b). I-V Characteristics of
coated and uncoated iron.

Resistivity of toroids was measured since magnetic loss measurements are done on toroid shape
samples. Equation employed for measurement of resistivity of toroid sample is given below [10].

ʹ ƒ ൈƒ
ρ ൌ 
ൈ ൌ 
(3)

Where, ρ is Resistivity (Ω m), V is Voltage developed across voltage probe at a distance of L cm

(v), I is Current supplied through current probes (A), a is cross sectional area (cm2), R is the resistance
of the toroid portion of length L and cross section a. I/2 is the current passing through half portion of
the toroid and it is passing through a uniform cross section area, a, of the toroid.

A Keithley nanovoltmeter was used for the measuring the voltage drop, V, between the voltage
sensing probes placed at a fixed distance, L, apart. A DC current of range of 100 to 1000 mA was
passed and I-V characteristics were plotted keeping the voltage probes distance at 0.5 cm. Figure 3
shows the schematic diagram of toroid sample for resistivity measurement and I-V characteristics of
coated and uncoated iron. The slope of the I-V graph gives the resistance R and equation (3) is used to
calculate resistivity. From the figure 3(b) the resistivity of coated iron is 280 μΩm, where as for
uncoated iron it is 0.2 μΩm.
3.3 DC & AC Magnetic properties

DC and AC hysteresis loops were recorded and core losses were measured on both uncoated and
coated iron powder toroids using B-H Loop tracer. Figure 4 and Figure 5 shows the DC and AC
hysteresis loops of uncoated iron powder and coated iron powder respectively. For uncoated iron the
hysteresis loops were distorted as the frequency increased, due to the eddy currents induced by AC
magnetic fields that opposes the applied field [11].

However for the coated iron due to its insulation on the surface the eddy current paths are limited
to within the iron particle itself. Thus eddy currents are minimal in the coated iron powder. Thus

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Study of AC magnetic properties and core losses ... Laxminarayana T. A. et al.

results in undistorted and nearly superposed hysteresis loops as a function of AC frequency. This can
be seen in the Figure 5. From figure 5 the superposition of the loops suggests that, the contribution of
eddy current losses are small and that there is a good electrical insulation amongst the particles.

Figure 4: DC & AC hysteresis loops of uncoated iron powder at the induction level of (a) 0.5 Tesla (b) 1
Tesla (colour online).

Figure 5: DC & AC hysteresis loops of coated iron powder at the induction level of (a) 0.5 Tesla (b) 1 Tesla
(colour online).

The relation between core loss and frequency is shown in figure 6 at various frequencies and
induction level of 0.5 Tesla and 1Tesla. For uncoated iron large change in core losses is seen due to
dominant eddy current losses at higher frequency. The core losses are seen to be non-linear with the
frequency. In the case of the coated iron due to its high resistivity, this relation is nearly linear, as eddy
current losses are much smaller in magnitude. Coated and uncoated iron annealed at 600˚C exhibited a
core loss of 91 W/kg and 693 W/kg respectively at 500 Hz and induction level of 1 Tesla.

The coated iron powder composite properties have been compared with the properties of a
commercially available sample Somaloy 130i-1P, a product of Hoganas, Sweden [12]. Table 1 shows
the comparison of properties between coated iron, uncoated iron and Somaloy130i-1P. Uncoated iron
annealed at 600ºC has high maximum permeability (µ max) and high magnetic induction due to the high
density obtained. The coated iron on the other hand has lesser maximum permeability and lesser
magnetic induction because of the insulation and pores present in the material. DC Induction value of
coated iron powder and Somaloy130i-1P at 10000 A/m are 1.35 Tesla and 1.4 Tesla respectively, with

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Study of AC magnetic properties and core losses ... Laxminarayana T. A. et al.

Core loss of 206 W/kg and 147 W/kg respectively at 1000 Hz and 1 Tesla. Utilization of the magnetic
nature of Fe3O4 in the insulation yielded properties similar to Somaloy130i-1P. Epoxy resin was used
in the composite to bind the nano Fe3O4 particles on to the iron powder.

Figure 6: Core losses of (a) uncoated iron and (b) coated iron powder at the induction level of 0.5 Tesla and 1
Tesla.

Table 1: Comparison of properties between coated iron, uncoated iron and Somaloy130i-1P.

Induction
@ Core Losses @ 1T [W/kg]
Density Resistivity 10000 µ max
Sample 100 500 1000
(g/cc) [μΩm] A/m
Hz Hz Hz
[Tesla]
Uncoated iron 7.6 0.2 1.60 1402 82 693 -
Coated iron 7.4 280 1.35 309 19 95 206
Somaloy130i-1P - 8000 1.40 290 12 54 145

4 Conclusion
A new method to prepare coated iron powder has been attempted. SEM images showed the
presence of uniform coating on iron powder. AC hysteresis loop studies of coated and uncoated iron
powder showed the effect of the insulation coating. The core losses, induction and permeability of
resulting coated iron were comparable with that of Somaloy130i-1P.

Acknowledgement

Authors are thankful to Prof. Veeturi Srinivas, Indian Institute of Technology, Madras for his
consistent support in the use of B-H Loop tracer available in his lab. Authors are also thankful to JFE
steel corporation, Tokyo, Japan for providing the atomized iron powder to work with. One of the
authors Laxminarayana T. A. thanks CSIR, Human Resource Development Group, India for the
research fellowship.

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